Formic Acid → HCID 21421756, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred mixture of 110 parts of (-)-2-[N-(1-phenylethyl)amino]acetonitrile and 1500 parts of dimethylbenzene are added dropwise 70 parts of formic acid (slightly exothermic reaction). Upon completion, stirring is continued first for 3 hours at reflux temperature (water-separator) and further over week-end (about 63 hours) at room temperature. The reaction mixture is heated to 60° C. and washed successively with water, a sodium bicarbonate solution, a diluted sodium hydroxide solution and again twice with water. The organic phase is separated, dried, filtered and evaporated. The residue is crystallized from a mixture of 80 parts of ethanol and 108 parts of 2,2'-oxybispropane. The product is filtered off and dried, yielding 46.5% of (-)-N-(cyanomethyl)-N-(1-phenylethyl)formamide; m.p. 78.8° C.; [α] = -60.7° (c = 1% CH3OH).

Provenance & Evidence